Synthetic method for cyclohexylamine
A synthesis method and technology of cyclohexylamine, applied in the preparation of nitrogen-oxygen/nitrogen-nitrogen bonds, organic chemistry, etc., can solve problems such as difficult operation, high production cost, and difficult application, and achieve mild reaction conditions and low production cost. The effect of low, high product purity
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Embodiment 1
[0012] Embodiment 1: a kind of synthetic method of cyclohexylamine, carries out following steps successively:
[0013] 1. Prepare a fresh Raney nickel (Raney Ni) catalyst (this is the prior art): 2g Ni-Al alloy is dissolved in 100mL sodium hydroxide aqueous solution containing 10g sodium hydroxide in batches until no bubbles are produced. Pour off the upper aqueous solution, wash with fresh distilled water several times, until the final wash is neutral.
[0014] 2. In a 500mL autoclave, 80mL (62.32g / 0.74mol) of cyclohexane was added sequentially, and all the above-prepared Raney
[0015] Ni and cyclohexanone oxime 113.2g (1.0mol). First replace the autoclave with hydrogen three times, and then fill it up to 3.0 MPa; then add 17 g (1.0 mol) of ammonia into the autoclave. Heat the above-mentioned mixture in the autoclave to 100°C for reduction reaction. During the reaction, the pressure drops, and hydrogen needs to be continuously replenished. Keep the pressure at 3.0MPa for h...
Embodiment 2
[0019] Embodiment 2: a kind of synthetic method of cyclohexylamine, carries out following steps successively:
[0020] 1, prepare fresh RaneyNi catalyst: with embodiment 1.
[0021] 2. In a 500mL autoclave, add water 100mL (100g / 5.56mol) and RaneyNi catalyst 3.0g (composed of 1.0g of fresh Raney Ni catalyst and 2.0g of Raney Ni catalyst in the filter cake recycled in Example 1) and 226.4 g (2.0 mol) of cyclohexanone oxime. Replace the autoclave twice with hydrogen, then fill it up to 1.0MPa, heat the above mixture in the autoclave to 150°C for reduction reaction, the pressure drops during the reaction, hydrogen needs to be continuously replenished, and hydrogenation is carried out under the condition of maintaining the pressure at 1.0MPa ; Until the hydrogen is no longer absorbed, the pressure is kept constant at this time, and the reaction time is 28h in total.
[0022] 3, with embodiment 1. The resulting cyclohexylamine yield reaches 55.7%. The total yield of the obtaine...
Embodiment 3
[0023] Embodiment 3: a kind of synthetic method of cyclohexylamine, carries out following steps successively:
[0024] 1, prepare fresh RaneyNi catalyst: with embodiment 1.
[0025] 2. Add 79.2 g (2.47 mol) of methanol, 10 g of fresh Raney Ni catalyst and 113.2 g (1.0 mol) of cyclohexanone oxime in sequence into a 500 mL autoclave. The autoclave was first replaced twice with hydrogen, and then filled to 5.0 MPa; and 17 g (1.0 mol) of liquid ammonia was added to the autoclave. Heat the above-mentioned mixture in the autoclave to 60°C for reduction reaction. During the reaction, the pressure drops, and hydrogen needs to be continuously replenished. Keep the pressure at 5.0MPa and hydrogenate; until no more hydrogen is absorbed, the pressure remains constant at this time, and the reaction time A total of 7h.
[0026] 3, with embodiment 1. The resulting cyclohexylamine yield reached 83.2%. The total yield of the obtained cyclohexylamine and dicyclohexylamine was 91.5%.
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